#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238837.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238837
loop_
_publ_author_name
'Suckert, Stefan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Bis(acetylacetonato-κ²O,O')(pyridine-κN)(thiocyanato-κN)manganese(III):
 a redetermination using data from a single crystal
;
_journal_coeditor_code           BT6942
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m657
_journal_paper_doi               10.1107/S1600536813030407
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Mn (C5 H7 O2)2 (N C S) (C5 H5 N)]'
_chemical_formula_moiety         'C16 H19 Mn N2 O4 S'
_chemical_formula_sum            'C16 H19 Mn N2 O4 S'
_chemical_formula_weight         390.33
_chemical_name_systematic
Bis(acetylacetonato-κ²O,O')(pyridine-κN)(thiocyanato-κN)manganese(III)
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8803(6)
_cell_length_b                   8.3195(5)
_cell_length_c                   15.9035(7)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.85
_cell_volume                     1836.49(16)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6523
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.8825
_exptl_absorpt_correction_T_min  0.8016
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.1718
_exptl_crystal_size_mid          0.1350
_exptl_crystal_size_min          0.0926
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.183
_refine_ls_abs_structure_details 'Flack (1983), 1086 Friedel pairs'
_refine_ls_abs_structure_Flack   0.015(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.9669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                2090
_reflns_number_total             2267
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6942.cif
_cod_data_source_block           I
_cod_database_code               2238837
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Mn Mn1 0.5000 0.70123(5) 0.26659(3) 0.03145(11) Uani d S 1 2
S S1 0.5000 1.19178(13) 0.09102(7) 0.0591(3) Uani d S 1 2
C C1 0.5000 1.0340(4) 0.1504(2) 0.0365(6) Uani d S 1 2
N N1 0.5000 0.9206(3) 0.19339(18) 0.0442(7) Uani d S 1 2
N N11 0.5000 0.4703(3) 0.35186(15) 0.0337(5) Uani d S 1 2
C C11 0.5000 0.4876(4) 0.4355(2) 0.0403(7) Uani d S 1 2
H H11 0.5000 0.5931 0.4583 0.048 Uiso calc SR 1 2
C C12 0.5000 0.3596(5) 0.4895(2) 0.0476(9) Uani d S 1 2
H H12 0.5000 0.3772 0.5485 0.057 Uiso calc SR 1 2
C C13 0.5000 0.2045(5) 0.4580(3) 0.0503(10) Uani d S 1 2
H H13 0.5000 0.1138 0.4943 0.060 Uiso calc SR 1 2
C C14 0.5000 0.1873(4) 0.3707(3) 0.0462(8) Uani d S 1 2
H H14 0.5000 0.0832 0.3461 0.055 Uiso calc SR 1 2
C C15 0.5000 0.3219(4) 0.3206(2) 0.0382(7) Uani d S 1 2
H H15 0.5000 0.3084 0.2613 0.046 Uiso calc SR 1 2
O O1 0.40265(11) 0.78003(17) 0.34197(9) 0.0387(3) Uani d . 1 1
O O2 0.40418(10) 0.60368(17) 0.19620(9) 0.0367(3) Uani d . 1 1
C C2 0.26139(19) 0.4840(3) 0.14949(17) 0.0528(6) Uani d . 1 1
H H2A 0.2535 0.5503 0.0990 0.079 Uiso calc R 1 1
H H2B 0.1979 0.4547 0.1716 0.079 Uiso calc R 1 1
H H2C 0.2972 0.3862 0.1352 0.079 Uiso calc R 1 1
C C3 0.31578(16) 0.5768(3) 0.21467(14) 0.0366(5) Uani d . 1 1
C C4 0.27229(17) 0.6295(3) 0.28825(14) 0.0453(6) Uani d . 1 1
H H4 0.2081 0.5956 0.2990 0.054 Uiso calc R 1 1
C C5 0.31605(15) 0.7284(3) 0.34724(15) 0.0397(5) Uani d . 1 1
C C6 0.2633(2) 0.7827(4) 0.42460(18) 0.0568(7) Uani d . 1 1
H H6A 0.3065 0.7769 0.4732 0.085 Uiso calc R 1 1
H H6B 0.2074 0.7130 0.4341 0.085 Uiso calc R 1 1
H H6C 0.2415 0.8938 0.4170 0.085 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Mn1 O2 . 4_655 87.77(9)
O2 Mn1 O1 . 4_655 174.74(7)
O2 Mn1 O1 4_655 4_655 91.20(6)
O2 Mn1 O1 . . 91.20(6)
O2 Mn1 O1 4_655 . 174.74(7)
O1 Mn1 O1 4_655 . 89.36(9)
O2 Mn1 N1 . . 92.46(8)
O2 Mn1 N1 4_655 . 92.46(8)
O1 Mn1 N1 4_655 . 92.74(7)
O1 Mn1 N1 . . 92.74(7)
O2 Mn1 N11 . . 89.47(6)
O2 Mn1 N11 4_655 . 89.47(6)
O1 Mn1 N11 4_655 . 85.36(6)
O1 Mn1 N11 . . 85.36(6)
N1 Mn1 N11 . . 177.31(11)
N1 C1 S1 . . 179.8(3)
C1 N1 Mn1 . . 176.6(3)
C15 N11 C11 . . 118.1(3)
C15 N11 Mn1 . . 122.9(2)
C11 N11 Mn1 . . 119.0(2)
N11 C11 C12 . . 122.7(3)
N11 C11 H11 . . 118.6
C12 C11 H11 . . 118.6
C11 C12 C13 . . 119.9(3)
C11 C12 H12 . . 120.0
C13 C12 H12 . . 120.0
C12 C13 C14 . . 117.1(4)
C12 C13 H13 . . 121.5
C14 C13 H13 . . 121.5
C15 C14 C13 . . 119.5(3)
C15 C14 H14 . . 120.2
C13 C14 H14 . . 120.2
N11 C15 C14 . . 122.7(3)
N11 C15 H15 . . 118.7
C14 C15 H15 . . 118.7
C5 O1 Mn1 . . 125.95(15)
C3 O2 Mn1 . . 127.15(14)
C3 C2 H2A . . 109.5
C3 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
C3 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
O2 C3 C4 . . 123.7(2)
O2 C3 C2 . . 114.5(2)
C4 C3 C2 . . 121.8(2)
C5 C4 C3 . . 124.5(2)
C5 C4 H4 . . 117.7
C3 C4 H4 . . 117.7
O1 C5 C4 . . 124.5(2)
O1 C5 C6 . . 114.3(2)
C4 C5 C6 . . 121.3(2)
C5 C6 H6A . . 109.5
C5 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C5 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O2 . 1.9185(15)
Mn1 O2 4_655 1.9185(15)
Mn1 O1 4_655 1.9216(15)
Mn1 O1 . 1.9216(15)
Mn1 N1 . 2.165(3)
Mn1 N11 . 2.352(2)
S1 C1 . 1.617(3)
C1 N1 . 1.165(4)
N11 C15 . 1.331(4)
N11 C11 . 1.338(4)
C11 C12 . 1.368(5)
C11 H11 . 0.9500
C12 C13 . 1.384(6)
C12 H12 . 0.9500
C13 C14 . 1.396(6)
C13 H13 . 0.9500
C14 C15 . 1.374(4)
C14 H14 . 0.9500
C15 H15 . 0.9500
O1 C5 . 1.279(3)
O2 C3 . 1.281(3)
C2 C3 . 1.497(3)
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C3 C4 . 1.388(3)
C4 C5 . 1.388(3)
C4 H4 . 0.9500
C5 C6 . 1.501(3)
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
